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Montmorillonite catalyst used in preparation of cyclic carbonate

A montmorillonite and catalytic system technology, applied in clean catalysis and green fields, can solve problems such as difficult separation, and achieve the effects of easy availability of raw materials, cheap raw materials and simple preparation

Inactive Publication Date: 2011-05-25
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

All these systems use ionic liquids directly for the reaction. Although the catalytic activity is high, the product after the reaction is miscible with the ionic liquid, and the separation is difficult, requiring further cumbersome steps such as distillation. Aiming at the current common problems, a greener, Catalysts that are easier to separate and can make the reaction conditions milder are necessary

Method used

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  • Montmorillonite catalyst used in preparation of cyclic carbonate
  • Montmorillonite catalyst used in preparation of cyclic carbonate
  • Montmorillonite catalyst used in preparation of cyclic carbonate

Examples

Experimental program
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example 1

[0028] Example 1: [C 4 {CH 2 COOH}im]Br Intercalation Modified Montmorillonite

[0029] Step 1. Preparation of Na-based montmorillonite: Take 3 g of montmorillonite raw soil (purified) and prepare it into a slurry. Add 3.5g NaCl to 20ml of deionized water, stir well to dissolve it completely, then fully mix the montmorillonite slurry with the prepared NaCl solution, stir in an oil bath at 80°C for 3 hours, complete a cation exchange process, and exchange three times continuously . After centrifugal dehydration, dry in an oven at 60° C. for 16 hours, and grind to obtain sodium-based montmorillonite.

[0030] Step 2, [C 4 {CH 2 COOH}im]Br ionic liquid preparation: 50mmol butylimidazole and 50mmol BrCH 2 COOCH 2 CH 3 Mixed, then heated slowly, and finally stirred and reacted for 8h in an oil bath at 50°C. After the reaction was over, the stirring was stopped and cooled, washed 3 times with ether, and then sucked dry. Then, in an oil bath at 70°C, hydrolyze with 10ml of ...

example 2

[0032] Example 2: [C 6 {CH 2 COOH}im]Br Intercalation Modified Montmorillonite

[0033] Step 1. Preparation of Na-based montmorillonite: Take 3 g of montmorillonite raw soil (purified) and prepare it into a slurry. Add 3.5g NaCl to 20ml of deionized water, stir well to dissolve it completely, then fully mix the montmorillonite slurry with the prepared NaCl solution, stir in an oil bath at 80°C for 3 hours, complete a cation exchange process, and exchange three times continuously . After centrifugal dehydration, dry in an oven at 60° C. for 16 hours, and grind to obtain sodium-based montmorillonite.

[0034] Step 2, [C 6 {(CH 2 )COOH}im]Br ionic liquid preparation: 50mmol hexylimidazole and 50mmol of BrCH 2 COOCH 2 CH 3 Mixed, then heated slowly, and finally stirred and reacted for 8h in an oil bath at 50°C. After the reaction was over, the stirring was stopped and cooled, washed 3 times with ether, and then sucked dry. Then in a 70°C oil bath, hydrolyze with 10ml of ...

example 3

[0036] Example 3: [C 8 {CH 2 COOH}im]Br Intercalation Modified Montmorillonite

[0037] Step 1. Preparation of Na-based montmorillonite: Take 3 g of montmorillonite raw soil (purified) and prepare it into a slurry. Add 3.5g NaCl to 20ml of deionized water, stir well to dissolve it completely, then fully mix the montmorillonite slurry with the prepared NaCl solution, stir in an oil bath at 80°C for 3 hours, complete a cation exchange process, and exchange three times continuously . After centrifugal dehydration, dry in an oven at 60° C. for 16 hours, and grind to obtain sodium-based montmorillonite.

[0038] Step 2, [C 8 {CH 2 Preparation of COOH}im]Br ionic liquid: 50mmol of octyl imidazole and 50mmol of BrCH 2 COOCH 2 CH 3 Mix, heat slowly, and stir for 8 hours in an oil bath at 50°C. After the reaction was completed, the stirring was stopped and cooled, washed 3 times with ether, and then sucked dry. Then in an oil bath at 70°C, hydrolyze with 10ml of 40% HBr for 2...

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Abstract

The invention relates to a natural montmorillonite catalyst which is modified by carboxyl functional ionic liquid and a preparation method thereof, and relates to a method for preparing cyclic carbonate by applying a catalyst system to a cycloaddition reaction of CO2 and an epoxy compound under the concerted catalysis action of quaternary ammonium salt. A method for preparing the catalyst comprises the following steps of: 1) treating the original montmorillonite to obtain sodium-based montmorillonite; 2) preparing the functional ionic liquid, namely synthesizing precursor of the carboxyl functional ionic liquid from alkyl imidazole and Br(CH2)mCOOCH2CH3, and performing hydrolysis with HBr to produce the carboxyl functional ionic liquid; and 3) performing a cation exchange process on the sodium-based montmorillonite and the functional ionic liquid in water to form ionic liquid intercalation modified montmorillonite. The prepared catalyst and different quaternary ammonium salts, which comprise tetrabutyl ammonium bromide, dodecyl trimethyl ammonium bromide and hexadecyl trimethyl ammonium bromide, are used for the concerted catalysis of the cycloaddition reaction of the CO2 and the epoxy compound. The catalyst has the advantages of simple preparation method, low raw material cost, high activity and high stability, and is suitable for the cycloaddition reaction of the CO2 and the epoxy compound.

Description

technical field [0001] The invention relates to the technical field of green and clean catalysis, in particular to a functional ionic liquid-modified natural montmorillonite catalytic system, and applies the prepared catalyst material to the reaction of preparing cyclocarbonate from carbon dioxide. [0002] The present invention also relates to the above catalytic system in CO 2 Application of cycloaddition reaction with epoxy compound to prepare cyclic carbonate. Background technique: [0003] Carbon dioxide is one of the main gases that cause the greenhouse effect. As the concentration of carbon dioxide in the atmosphere continues to rise, it not only intensifies the greenhouse effect, but also poses a potential threat to the global ecological environment. In fact, carbon dioxide is a valuable carbon source. It is widely distributed and abundant in reserves. It is one of the cheapest carbon resources. It also has many properties such as stable, non-toxic, non-corrosive, a...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07D319/06
Inventor 侯震山曹婷王明洁孙立婷张璐琳石玉
Owner EAST CHINA UNIV OF SCI & TECH
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